Dispersive liquid-liquid microextraction method of heavy metal ions by using alkyl carboxylic acid as extracting agent
A technology of heavy metal ions and alkyl carboxylic acids, applied in liquid solution solvent extraction, preparation of test samples, etc., can solve problems such as limited types of chelating agents and chelating efficiency, poor stability of chelating agents, and increased method complexity. Achieve the effect of low cost, less organic solvent and simple device
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Embodiment 1
[0036] Use mercuric chloride or mercuric nitrate crystals to configure Hg concentrations of 0, 1.0, 2.0, 4.0, 6.0, 8.0, 10.0ppb (micrograms per liter) respectively 2+ Aqueous solutions (respectively as standard samples) were enriched by using dispersion liquid-liquid microextraction method, the steps are as follows: first add 200mL Hg 2+ For the standard sample, heat the sample to 50°C and adjust the pH to 5; pre-mix 150 μL dodecanoic acid extractant and 3 mL methanol dispersant; quickly inject the mixed dodecanoic acid and methanol into the sample with a syringe to Stir rapidly at 1000r / min for 2min to form an emulsified system; place the sample in an ice bath for 10min; filter and separate the solidified dodecanoic acid; add 1mL of methanol to dissolve all the separated dodecanoic acid, and then add 2mL of 500μM rhodamine B Derivative rhodamine B thiospirolactone in acetonitrile solution, mixed well and then detected by fluorescence spectrometer.
[0037] Spectral condition...
Embodiment 2
[0039] Use nickel chloride crystals to configure Ni with concentrations of 50.0, 100.0, 150.0, 200.0, 250.0, 300.0, 350.0, 400.0ng / L 2+ Aqueous solutions (respectively used as water samples) were enriched by dispersion liquid-liquid microextraction method. The steps are as follows: first, add 100mL water sample to the extraction bottle, and place the extraction bottle in a water bath at 40°C; Mix with ethanol, quickly pour the mixture into the extraction bottle with a pipette, shake for 5 minutes, place the extraction bottle in an ice bath for 5 minutes, filter and separate n-decanoic acid; heat to 40°C, melt the extraction phase to obtain 150 μL n-decanoic acid, 20 μL was injected into electrothermal atomic absorption spectroscopy (ETAAS) for analysis. The initial concentration Caq of nickel ions in the aqueous phase sample was plotted against the concentration Cor of nickel ions in the 150 μL n-decanoic acid extraction phase separated by filtration. It was found that the lin...
Embodiment 3
[0041]Pb with concentration of 20.0, 60.0, 100.0, 140.0, 180.0, 220.0, 260.0ng / L is prepared with lead chloride crystal 2+ Aqueous solutions (respectively used as water samples) were enriched by using dispersion liquid-liquid microextraction method, the steps are as follows: first, add 100mL water sample to the extraction bottle, and place the extraction bottle in a water bath at 30°C; Mix with acetone, quickly inject the mixture into the extraction bottle with a syringe, and stir rapidly at 1000r / min for 2 minutes to form an emulsified system; place the extraction bottle in an ice bath for 5 minutes, filter and separate the extract phase and heat to 30°C to obtain 150 μL n-nonyl acid; 15 μL was injected into atomic fluorescence spectroscopy (AFS) for analysis. The method for Pb 2+ The enrichment factor is 350 times and the detection limit can reach 10ng / L. The peak height has a good linear relationship with the sample concentration in the concentration range of 20-260ng / L.
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